We report a new low temperature method for the synthesis of LnNiO 3 (Ln = Eu, Gd) at 400 °C under 180 bar oxygen pressure with the flux method. Utilization of the LiCl/KCl flux allowed for a decrease of the reaction temperature from 1000 °C and resulted in the synthesis of pure phase compounds. These materials have been characterized by powder X-ray diffraction and thermogravimetric analysis. LnNiO3 (Ln = Eu and Gd) compounds crystallize in the orthorhombic GdFeO3-type perovskite structure (space group: Pbnm). Both materials decompose to Ln2O 3 and NiO at 775 °C under a nitrogen atmosphere and undergo reduction to Ln2O3 and Ni metal (at 385 °C and 340 °C for Eu and Gd, respectively) under a hydrogen atmosphere (10% H 2/N2). Attempts to prepare the first T′-type infinite layer compound with Ni2+, EuNiO2, by low temperature reduction of EuNiO3 were unsuccessful. © 2012 Elsevier Masson SAS. All rights reserved.